CN105060311B - A kind of preparation method of the water-fast silica gel of hydrophilic radical bonding - Google Patents
A kind of preparation method of the water-fast silica gel of hydrophilic radical bonding Download PDFInfo
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- CN105060311B CN105060311B CN201510524144.1A CN201510524144A CN105060311B CN 105060311 B CN105060311 B CN 105060311B CN 201510524144 A CN201510524144 A CN 201510524144A CN 105060311 B CN105060311 B CN 105060311B
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Abstract
The present invention relates to a kind of preparation method of the water-fast silica gel of hydrophilic radical bonding, using waterglass and sulfuric acid as initial feed, by gel, acidification, aging, washing, reaming, silica gel is dried to obtain；Silica gel with intermediate reaction by obtaining hydrophilic radical bonded silica gel, then process washing, dry, end product packaging.The water-fast silica gel for the hydrophilic radical bonding that the present invention is made（Modified water-fast silica gel）, the bonding of a small amount of hydrophilic radical can slow down silica gel to the water drastically rate of adsorption, and surface tension during reduction silica gel absorption water, so that silica gel internal stress reduces, reaches that chance water does not split, particle percentage of head rice is significantly improved, and effectively increases the water resistance of silica gel.
Description
Technical field
Field is made the invention belongs to silica gel, and in particular to a kind of preparation method of the water-fast silica gel of hydrophilic radical bonding.
Background technology
Common silica gel has open loose structure, and larger specific surface area can adsorb many kinds of substance, is a kind of good
Drier, adsorbent and catalyst carrier, but its meet water easily burst so that particle percentage of head rice decline, influence silica gel it is normal
Use.
Common silica gel meets the main cause that water easily splits：Because frame strength is insecure, pore size distribution is uneven, if silica gel particle
The a large amount of water of absorption in short time, the distribution and pore size due to particle hole is different, and the speed difference of water suction causes each position
Expansion rate is different, and silica gel solid grain structure can not shrink amplification therewith, will be burst under stress.In order that silica gel
Possess preferable water resistance, mainly set about in terms of two：1st, the frame strength of silica gel, surface during reduction adsorption desorption water are increased
The influence of power, granule strength is strengthened by adding the reinforcing agents such as titanium, aluminium；2nd, by carrying out moditied processing, key to Silica Surface
Enter organic functions active group, these groups are hydrophilic radicals, but also there is certain hydrophobicity, silica gel can be slowed down anxious to water
The acute rate of adsorption, reduces surface tension during silica gel absorption water, so that silica gel internal stress reduces, preferably protects silica gel bone
Frame structure.
In early days, the production technology of domestic water-fast silica gel, is mainly mixed using silica gel powder with inorganic or organic bond
Shaping, is formed, this method is inconvenient to adjust the pore-size distribution of silica gel, is gradually eliminated through high-temperature calcination.At present, it is solidifying using sial
Glue method prepares the compound water-resistant material of sial, and silica gel product water resistance prepared by this method is good, and such product is generally used for work
In terms of industry, the acetylene absorption in being air-dried in air separation process, liquid oxygen, liquid nitrogen preparation process is mainly used in, in stone
Make liquid absorbent etc. in oiling work, but because this water-resistant material contains more aluminium component, thus, it is in civilian, daily side
Face is using less.
Therefore, develop and develop it is a kind of be modified water-fast silica gel there is certain realistic meaning, its market is using wide, especially
Had a good application prospect at civilian, daily aspect.
The content of the invention
It is an object of the invention to provide a kind of water-fast silica gel of hydrophilic radical bonding（Modified water-fast silica gel）Preparation side
Method, by keying in organic functions active group to Silica Surface, these groups are hydrophilic radicals, but also have certain hydrophobic
Property, silica gel can be slowed down to the water drastically rate of adsorption, surface tension during reduction silica gel absorption water, so that silica gel internal stress subtracts
It is small, reach that chance water does not split, particle percentage of head rice is significantly improved.The present invention is achieved through the following technical solutions：
A kind of preparation of the water-fast silica gel of hydrophilic radical bonding, comprises the following steps：
（1）Using waterglass and sulfuric acid as initial feed, by gel, acidification, aging, washing, reaming, it is dried to obtain
Silica gel；
（2）The preparation of intermediate：The intermediate is gamma-amino propyl trimethoxy silicane, is used with γ-chloropropyl three
Methoxy silane is that raw material reacts with liquefied ammonia, gamma-amino propyl trimethoxy silicane is made, equipped with heating mantle, electric stirring
30mL toluene, 0.1 mol γ-r-chloropropyl trimethoxyl silicon are sequentially added in device, thermometer, the autoclave of reflux condenser
Alkane, reacts under agitation, is slowly introducing liquefied ammonia, and reaction temperature gradually rises, and controls at 70-80 DEG C, when being passed through liquid again
Ammonia is when the temperature drops, stop being passed through liquefied ammonia, continuation is stirred 30 minutes, and then decompression steams gamma-amino propyl trimethoxy silicane；
Chemical equation is：As shown in Figure 2；
（3）Silica gel obtains hydrophilic radical bonded silica gel, the hydrophilic radical bonded silica gel also known as modification with intermediate reaction
Water-fast silica gel, takes the silica gel (42.8 g) of certain granules degree to be placed in reactor, adds 80mL toluene, 0.5 gram of gamma-amino
Propyl trimethoxy silicane, heating stirring backflow 3-4h, after reaction terminates, filters out solid matter, successively in nitrogen atmosphere
With methanol, water washing for several times, it is dried in vacuo at room temperature, obtains hydrophilic radical and be bonded water-fast silica gel；Chemical equation is：Such as Fig. 3
It is shown；
（4）Hydrophilic radical bonded silica gel is scrubbed, be dried to obtain finished product；
（5）Product is through after the assay was approved, carrying out packaging and storage.
Beneficial effects of the present invention：The water-fast silica gel for the hydrophilic radical bonding that the present invention is made（Modified water-fast silica gel）, it is few
The bonding of hydrophilic radical is measured, silica gel can be slowed down to the water drastically rate of adsorption, surface tension during reduction silica gel absorption water, so that
Silica gel internal stress reduces, and reaches that chance water does not split, particle percentage of head rice is significantly improved, and effectively increases the water resistance of silica gel.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of the preparation for the water-fast silica gel that hydrophilic radical is bonded；
Fig. 2 is the chemical equation that gamma-amino propyl trimethoxy silicane is made；
Fig. 3 is that hydrophilic radical is made to be bonded water-fast silica gel chemical equation.
Embodiment
A kind of preparation of the water-fast silica gel of hydrophilic radical bonding, comprises the following steps：
（1）Using waterglass and sulfuric acid as initial feed, by gel, acidification, aging, washing, reaming, it is dried to obtain
Silica gel；
（2）The preparation of intermediate：The intermediate is gamma-amino propyl trimethoxy silicane, is used with γ-chloropropyl three
Methoxy silane is that raw material reacts with liquefied ammonia, gamma-amino propyl trimethoxy silicane is made, equipped with heating mantle, electric stirring
30mL toluene, 0.1 mol γ-r-chloropropyl trimethoxyl silicon are sequentially added in device, thermometer, the autoclave of reflux condenser
Alkane, reacts under agitation, is slowly introducing liquefied ammonia, and reaction temperature gradually rises, and controls at 80 DEG C, when being passed through liquefied ammonia again
When the temperature drops, stopping being passed through liquefied ammonia, continue to stir 30 minutes, then decompression steams gamma-amino propyl trimethoxy silicane；Change
Learning reaction equation is：As shown in Figure 2；
（3）Silica gel obtains hydrophilic radical bonded silica gel, the hydrophilic radical bonded silica gel also known as modification with intermediate reaction
Water-fast silica gel, takes the silica gel of 42.8 g certain granules degree to be placed in reactor, adds 80mL toluene, 0.5 gram of gamma-amino third
Base trimethoxy silane, heating stirring backflow 4h, after reaction terminates, filters out solid matter, first is used successively in nitrogen atmosphere
Alcohol, water washing for several times, are dried in vacuo at room temperature, are obtained hydrophilic radical and are bonded water-fast silica gel；Chemical equation is：As shown in Figure 3；
（4）Hydrophilic radical bonded silica gel is scrubbed, be dried to obtain finished product；
（5）Product is through after the assay was approved, carrying out packaging and storage.
Technical indicator：
（1）Micropore volume requirement is in 0.2-1.8 ml/g；
（2）Average pore size requirement is in 20-180；
（3）Specific surface area requirement is in 280-700m2/g；
（4）Silica gel particle 1-4mm；
（5）Hydrophilic radical is bonded coverage rate 2-7% on Silica Surface.
Claims (1)
1. a kind of preparation of the water-fast silica gel of hydrophilic radical bonding, it is characterised in that comprise the following steps：
（1）Using waterglass and sulfuric acid as initial feed, by gel, acidification, aging, washing, reaming, silicon is dried to obtain
Glue；
（2）The preparation of intermediate：The intermediate is gamma-amino propyl trimethoxy silicane, is used with γ-chloropropyl trimethoxy
Base silane is that raw material reacts with liquefied ammonia, gamma-amino propyl trimethoxy silicane is made, equipped with heating mantle, electric mixer, temperature
30mL toluene, 0.1 mol γ-r-chloropropyl trimethoxyl silane are sequentially added in degree meter, the autoclave of reflux condenser,
Reacted under stirring condition, be slowly introducing liquefied ammonia, reaction temperature gradually rises, controlled at 70-80 DEG C, when being passed through liquefied ammonia temperature again
When degree declines, stopping is passed through liquefied ammonia, continues to stir 30 minutes, then decompression steams gamma-amino propyl trimethoxy silicane；
（3）Silica gel obtains hydrophilic radical bonded silica gel with intermediate reaction, and the hydrophilic radical bonded silica gel also known as modification are water-fast
Silica gel, takes 42.8 g silica gel to be placed in reactor, addition 80mL toluene, 0.5 gram of gamma-amino propyl trimethoxy silicane,
Heating stirring backflow 3-4h, after reaction terminates, filters out solid matter in nitrogen atmosphere, successively with methanol, water washing for several times,
It is dried in vacuo at room temperature, obtains hydrophilic radical and be bonded water-fast silica gel；
（4）Hydrophilic radical bonded silica gel is scrubbed, be dried to obtain finished product；
（5）Product is through after the assay was approved, carrying out packaging and storage.
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| CN201510524144.1A CN105060311B (en) | 2015-08-25 | 2015-08-25 | A kind of preparation method of the water-fast silica gel of hydrophilic radical bonding |
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| CN105060311B true CN105060311B (en) | 2017-08-25 |
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| JP4769927B2 (en) * | 2004-04-22 | 2011-09-07 | 富士化学株式会社 | Method for producing silica adsorbent |
| CN1864852B (en) * | 2006-04-19 | 2012-01-11 | 南昌大学 | A method for preparing chromatogram stationery phase of rhein bonded silica gel |
| CN101785991B (en) * | 2009-12-12 | 2012-08-29 | 鲁东大学 | Preparation method of amino bonded silica gel glycerol adsorbent and prepared product thereof |
| CN102086309A (en) * | 2010-04-03 | 2011-06-08 | 兰州交通大学 | Preparation method of modified inorganic nanoparticle grafted by polymers through esterification at room temperature |
| CN104073215A (en) * | 2014-06-30 | 2014-10-01 | 江苏华程光电科技有限公司 | Preparation method for nano silicon dioxide modified organic silicon sealant for packaging of light emitting diode (LED) |
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